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Effect of plasma surface treatment of poly(dimethylsiloxane) on the permeation of pharmaceutical compounds

Waters J. LAURA ; Finch V. CATHERINE ; Hemming KARL ; Mitchell C. JOHN

Journal of Pharmaceutical Analysis.2017;7(5):338-342.

This paper addresses the modification of poly(dimethylsiloxane), i.e. PDMS, using plasma surface treatment and a novel application of the membrane created. A set of model compounds were analysed to determine their permeation through PDMS, both with and without plasma treatment. It was found that plasma treatment reduced permeation for the majority of compounds but had little effect on some compounds, such as caffeine, with results indicating that polarity plays an important role in permeation, as is seen in human skin. Most importantly, a direct correlation was observed between plasma-modified permeation data and literature data through calculation of membrane permeability (Kp) values suggesting plasma-modified silicone membrane (PMSM) could be considered as a suitable in vivo replacement to predict clinical skin permeation.

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In-depth investigation on physicochemical and thermal properties of magnesium (II) gluconate using spectroscopic and thermoanalytical techniques

Trivedi Kumar MAHENDRA ; Dixit NEENA ; Panda PARTHASARATHI ; Sethi Kumar KALYAN ; Jana SNEHASIS

Journal of Pharmaceutical Analysis.2017;7(5):332-337.

Magnesium gluconate is a classical organometallic pharmaceutical compound used for the prevention and treatment of hypomagnesemia as a source of magnesium ion. The present research described the in-depth study on solid state properties viz. physicochemical and thermal properties of magnesium gluconate using sophisticated analytical techniques like Powder X-ray diffraction (PXRD), particle size analysis ( PSA), Fourier transform infrared (FT-IR) spectrometry, ultraviolet–visible (UV–Vis) spectroscopy, thermogravimetric analysis (TGA)/differential thermogravimetric analysis (DTG), and differential scanning calorimetry (DSC). Magnesium gluconate was found to be crystalline in nature along with the crystallite size ranging from 14.10 to 47.35 nm. The particle size distribution was at d(0.1)=6.552 μm, d(0.5)=38.299 μm, d(0.9)=173.712 μm and D(4,3)=67.122 μm along with the specific surface area of 0.372 m2/g. The wavelength for the maximum absorbance was at 198.0 nm. Magnesium gluconate exhibited 88.51% weight loss with three stages of thermal degradation process up to 895.18 ℃ from room temperature. The TGA/DTG thermograms of the analyte indicated that magnesium gluconate was thermally stable up to around 165 ℃. Consequently, the melting temperature of magnesium gluconate was found to be 169.90 ℃ along with the enthalpy of fusion of 308.7 J/g. Thus, the authors conclude that the achieved results from this study are very useful in pharmaceutical and nutraceutical industries for the identification, characterization and qualitative analysis of magnesium gluconate for preformulation studies and also for developing magnesium gluconate based novel formulation.

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Identification of botanical origin of Chinese unifloral honeys by free amino acid profiles and chemometric methods

Sun ZHENG ; Zhao LINGLING ; Cheng NI ; Xue XIAOFENG ; Wu LIMING ; Zheng JIANBIN ; Cao WEI

Journal of Pharmaceutical Analysis.2017;7(5):317-323.

The amino acid contents of five floral sources Chinese honeys (jujube, rape, chaste, acacia, and lungan) were measured using reversed phase high-performance liquid chromatography (RP-HPLC). The results showed that proline was the main amino acid in most of the analyzed samples. Phenylalanine presents at the highest content in chaste honey samples, and the total amino acid contents of chaste honeys were also significantly higher than those of other honey samples. Based on the amino acid contents, honey samples were classified using chemometric methods (cluster analysis (CA), principal component analysis (PCA), and discriminant analysis (DA)). According to the CA results, chaste honeys could be separated from other honeys, while the remaining samples were correctly grouped together when the chaste honey data were excluded. By using DA, the overall correct classification rate reached 100%. The results revealed that amino acid contents could potentially be used as indicators to identify the botanical origin of unifloral honeys.

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Separation and determination of acetyl-glutamine enantiomers by HPLC–MS and its application in pharmacokinetic study

Zhang XIAOXIAO ; Gao LEI ; Zhang ZUNJIAN ; Tian YUAN

Journal of Pharmaceutical Analysis.2017;7(5):303-308.

A high-performance liquid chromatography coupled with mass spectrometry (HPLC–MS) method was established for the separation and determination of acetyl-glutamine enantiomers (acetyl-L-glutamine and acetyl-D-glutamine) simultaneously. Baseline separation was achieved on Chiralpak AD-H column (250 mm × 4.6 mm, 5 μm). n-Hexane (containing 0.1% acetic acid) and ethanol (75:25, v/v) were used as mobile phase at a flow rate of 0.6 mL/min. The detection was operated in the negative ion mode with an ESI source. [M-H]? m/z 187.0540 for enantiomers and [M-H]? m/z 179.0240 for aspirin (IS) were selected as detecting ions. The linear range of the calibration curve for each enantiomer was 0.05–40 μg/mL. The precision of this method at concentrations of 0.5–20 μg/mL was within 7.23%, and the accuracy was 99.81%–107.81%. The precision at LOQ (0.05 μg/mL) was between 16.28% and 17.56%, which was poor than that at QC levels. The average extraction recovery was higher than 85% for both enantiomers at QC levels. The pharmacokinetics of enantiomers was found to be stereoselective. There was not chiral inversion in vivo or in vitro between enantiomers.

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Degradation rates and products of fluticasone propionate in alkaline solutions

Tokumura TADAKAZU ; Yoshida NAOKO ; Yasumoto Mori KANAMI ; Shirota OSAMU ; Kurita TAKURO

Journal of Pharmaceutical Analysis.2017;7(5):297-302.

The apparent degradation rate constant of fluticasone propionate (FLT) in 0.1 M NaOH:methanol=1:1 at 37 ℃ was previously reported to be 0.169 ± 0.003 h?1, and four degradation products (products 1–4) were observed in the solution. The aims of the present study were to assess the degradation rates of FLT in other alkaline solutions and clarify the chemical structures of the four degradation products in order to obtain basic data for designing an enema for inflammatory bowel disease. The apparent degradation rate constants in 0.05 M NaOH and 0.1 M NaOH:CH3CN=1:1 were 0.472 ± 0.013 h?1 and 0.154 ± 0.000 h?1 (n=3), respectively. The chemical structures of products 1–4 in 0.1 M NaOH:methanol=1:1 were revealed by nuclear magnetic resonance (NMR) and mass spectrometry data. The chemical structure of products 2 was that the 17-position of the thioester moiety of FLT was substituted by a carboxylic acid. The degradation product in 0.1 M NaOH:CH3CN=1:1 was found to be product 2 based on 1H NMR data. The degradation product in 0.05 M NaOH was considered to be product 2 based on the retention time of HPLC. These results are useful for detecting the degradation products of FLT by enzymes of the intestinal bacterial flora in the large intestine after dosing FLT as an enema.

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Chemical and microbiological characterization of tinctures and microcapsules loaded with Brazilian red propolis extract

Kamiya Umeko REGIANNE ; Vieira Abreu DANILO ; Escodro Barnabé PIERRE ; Basílio-Júnior Diniz IRINALDO

Journal of Pharmaceutical Analysis.2017;7(5):280-287.

The aim of this study was to characterize tinctures and microcapsules loaded with an ethanol extract of red propolis through chemical, physicochemical and microbiological assays in order to establish quality control tools for nutraceutical preparations of red propolis. The markers (isoflavonoids, chalcones, pterocarpans, flavones, phenolic acids, terpenes and guttiferones) present in the tinctures A and B were identified and confirmed using LC/ESI/FTMS/Orbitrap. Four compositions (A, B, C and D) were prepared to contain B tincture of the red propolis with some pharmaceutical excipients and submitted to two drying processes, i. e. spray-drying and freeze-drying to obtain microcapsules loaded with the red propolis extract. The tinctures and microcapsules of the red propolis were submitted to the total flavonoid content and antioxidant activity tests. The antibacterial activity and minimum inhibitory concentration (MIC) were tested using Staphylococcus aureus ATCC 25293 and Pseudomonas aeruginosa ATCC 27853 strains. The tinctures and microcapsules presented high flavonoid quantities from 20.50 to 40.79 mg/100 mg of the microcapsules. The antioxidant activity and IC50 were determined for the tinctures A and B (IC50: 6.95 μg/mL and 7.48 μg/mL), the spray-dried microcapsules (IC50: 8.89–15.63 μg/mL) and the freeze-dried microcapsules (IC50: 11.83–23.36 μg/mL). The tinctures and microcapsules were proved to be bioactive against gram-positive and gram-negative bacteria with inhibition halos superior to 10 mm at concentration of 200 μg/mL and MIC values of 135.87–271.74 μg/mL using gram-positive strain and 271.74–543.48 μg/mL using gram-negative strain. The tinctures and microcapsules of the red propolis have a potential application for nutraceutical products.

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A holistic strategy for quality and safety control of traditional Chinese medicines by the"iVarious"standard system

Chen ANZHEN ; Sun LEI ; Yuan HANG ; Wu AIYING ; Lu JINGGUANG ; Ma SHUANGCHENG

Journal of Pharmaceutical Analysis.2017;7(5):271-279.

An effective quality control system is the key to ensuring the quality, safety and efficacy of traditional Chinese medicines (TCMs). However, the current quality standard research lacks top-level design and systematic design, mostly based on specific technologies or evaluation methods. To resolve the challenges and questions of quality control of TCMs, a brand-new quality standard system, named "iVarious", was proposed. The system comprises eight elements in a modular format. Meaning of every element was specifically illustrated via corresponding research instances. Furthermore, frankincense study was taken as an example for demonstrating standards and research process, based on the "iVarious" system. This system highlighted a holistic strategy for effectiveness, security, integrity and systematization of quality and safety control standards of TCMs. The establishment of "iVarious" integrates multi-disciplinary technologies and progressive methods, basis elements and key points of standard construction. The system provides a novel idea and technological demonstration for regulation establishment of TCMs quality standards.

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Isolation, characterization and chromatography based purification of antibacterial compound isolated from rare endophytic actinomycetes Micrococcus yunnanensis

Ranjan RAVI ; Jadeja VASANTBA

Journal of Pharmaceutical Analysis.2017;7(5):343-347.

Endophytic actinomycetes are considered as one of the relatively unexplored potential sources in search of antibiotic producer against antibiotic resistant pathogens. A potent strain isolated from Catharanthus roseus that displays antibacterial potential against antibiotic resistant human pathogen Staphylococcus aureus was characterized and designated as Micrococcus yunnanensis strain rsk5. Rsk5 is capable of producing optimum antibacterial metabolites on starch casein medium at 30 ℃, pH 5 and 2% NaCl condition. The crude antibacterial agent was extracted from fermentation broth by ethyl acetate and separated by TLC using chloroform-methanol (24:1, v/v) solvent system with Rf value of 0.26. It was partially purified by flash chromatography, followed by HPLC and analyzed by ultraviolet visible spectrophotometer to get absorption maxima at 208.4 nm. The ESI-MS spectra showed molecular ion peaks at m/z 472.4 [M-H], which does not match with any known antibacterial compound.

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Analysis of penicillamine using Cu-modified graphene quantum dots synthesized from uric acid as single precursor

Durán M. GEMA ; Benavidez E. TOMÁS ; Contento M. ANA ; Ríos ANGEL ; García D. CARLOS

Journal of Pharmaceutical Analysis.2017;7(5):324-331.

A simple methodology was developed to quantify penicillamine (PA) in pharmaceutical samples, using the selective interaction of the drug with Cu-modified graphene quantum dots (Cu-GQDs). The proposed strategy combines the advantages of carbon dots (over other nanoparticles) with the high affinity of PA for the proposed Cu-GQDs, resulting in a significant and selective quenching effect. Under the optimum conditions for the interaction, a linear response (in the 0.10–7.50 μmol/L PA concentration range) was observed. The highly fluorescent GQDs used were synthesized using uric acid as single precursor and then characterized by high resolution transmission electron microscopy, Raman spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy, fluorescence, and absorption spectroscopy. The proposed methodology could also be extended to other compounds, further expanding the applicability of GQDs.

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Application of an LC–MS/MS method for the analysis of amlodipine, valsartan and hydrochlorothiazide in polypill for a bioequivalence study

Shah V. JAIVIK ; Parekh M. JIGNESH ; Shah A. PRIYANKA ; Shah V. PRIYA ; Sanyal MALLIKA ; Shrivastav S. PRANAV

Journal of Pharmaceutical Analysis.2017;7(5):309-316.

A sensitive and selective method has been proposed for the simultaneous determination of amlodipine (AML), valsartan (VAL) and hydrochlorothiazide (HCTZ) in human plasma by liquid chromatography–tandem mass spectrometry (LC–MS/MS). The analytes and their deuterated analogs were quantitatively extracted from 100 μL human plasma by solid phase extraction on Oasis HLB cartridges. The chromatographic separation of the analytes was achieved on a Chromolith RP18e (100 mm × 4.6 mm) analytical column within 2.5 min. The resolution factor between AML and VAL, AML and HCTZ, and VAL and HCTZ was 2.9, 1.5 and 1.4, respectively, under isocratic conditions. The method was validated over a dynamic concentration range of 0.02–20.0 ng/mL for AML, 5.00–10,000 ng/mL for VAL and 0.20–200 ng/mL for HCTZ. Ion-suppression/enhancement effects were investigated by post-column infusion technique. The mean IS-normalized matrix factors for AML, VAL and HCTZ were 0.992, 0.994 and 0.998, respectively. The intra-batch and inter-batch precision (% CV) across quality control levels was ≤ 5.56% and the recovery was in the range of 93.4%–99.6% for all the analytes. The method was successfully applied to a bioequivalence study of 5 mg AML + 160 mg VAL + 12.5 mg HCTZ tablet formulation (test and reference) in 18 healthy Indian males under fasting. The mean log-transformed ratios of Cmax, AUC0–120h and AUC0-inf and their 90% CIs were within 90.2%–102.1%. The assay reproducibility was demonstrated by reanalysis of 90 incurred samples.

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